EP2707540B1 - Verfahren zur behandlung mikrofibrillierter cellulose und in diesem verfahren behandelte mikrofibrillierte cellulose - Google Patents

Verfahren zur behandlung mikrofibrillierter cellulose und in diesem verfahren behandelte mikrofibrillierte cellulose Download PDF

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Publication number
EP2707540B1
EP2707540B1 EP12786645.7A EP12786645A EP2707540B1 EP 2707540 B1 EP2707540 B1 EP 2707540B1 EP 12786645 A EP12786645 A EP 12786645A EP 2707540 B1 EP2707540 B1 EP 2707540B1
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European Patent Office
Prior art keywords
slurry
microfibrillated cellulose
dewatering
process according
cellulose
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EP12786645.7A
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English (en)
French (fr)
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EP2707540A1 (de
EP2707540A4 (de
Inventor
Isto Heiskanen
Kaj Backfolk
Ari KOTILAINEN
Valentas Gaidelis
Jonas Sidaravicius
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Stora Enso Oyj
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Stora Enso Oyj
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Classifications

    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/18—De-watering; Elimination of cooking or pulp-treating liquors from the pulp
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/42—Electrodialysis; Electro-osmosis ; Electro-ultrafiltration; Membrane capacitive deionization
    • B01D61/56—Electro-osmotic dewatering
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/006—Electrochemical treatment, e.g. electro-oxidation or electro-osmosis
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21C—PRODUCTION OF CELLULOSE BY REMOVING NON-CELLULOSE SUBSTANCES FROM CELLULOSE-CONTAINING MATERIALS; REGENERATION OF PULPING LIQUORS; APPARATUS THEREFOR
    • D21C9/00—After-treatment of cellulose pulp, e.g. of wood pulp, or cotton linters ; Treatment of dilute or dewatered pulp or process improvement taking place after obtaining the raw cellulosic material and not provided for elsewhere
    • D21C9/001—Modification of pulp properties
    • D21C9/007—Modification of pulp properties by mechanical or physical means
    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • D21H11/16—Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only modified by a particular after-treatment
    • D21H11/18—Highly hydrated, swollen or fibrillatable fibres
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4698—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis electro-osmosis
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/12—Treatment of sludge; Devices therefor by de-watering, drying or thickening
    • C02F11/15—Treatment of sludge; Devices therefor by de-watering, drying or thickening by treatment with electric, magnetic or electromagnetic fields; by treatment with ultrasonic waves

Definitions

  • the present invention relates to a process for dewatering, a slurry comprising microfibrillated cellulose by subjecting the slurry to an electric field.
  • Microfibrillated cellulose which also is known as nanocellulose, is a material typically made from wood cellulose fibers. It can also be made from microbial sources, agricultural fibers, dissolved cellulose or CMC etc. In microfibrillated cellulose the individual microfibrils have been partly or totally detached from each other.
  • Microfibrillated cellulose has a very high water binding capacity and it is thus very difficult to reduce the water content of a slurry comprising microfibrillated cellulose.
  • High water content of a slurry comprising microfibrillated cellulose also prevents usage of MFC in many different application where MFC with high solids would be required.
  • the hornification may be prevented by addition of chemicals which physically prevent or modify the fibers in such way that the formation of bonds between cellulose fibers are limited or prevented.
  • CA1208631A describes a process to re-disperse dried microfibrillated cellulose by addition of additives that will prevent the fibrils from bonding to each other and thus also prevents hornification of the fibers.
  • EP 2196579 A1 describes a method for producing MFC by passing a cellulose fibre suspension through a homogenizer.
  • the solvent/liquid is removed from the suspension/slurry containing MFC by methods such as evaporation, spray-drying, cross-flow filtration, pressing, freeze drying, etc.
  • the present invention solves one or more of the above problems, by providing according to a first aspect a process for dewatering of a slurry comprising microfibrillated cellulose wherein the process comprises the following steps:
  • the present invention also provides according to a second aspect microfibrillated cellulose dewatered according to the first aspect.
  • the present invention also provides according to a third aspect, microfibrillated cellulose obtainable by the process according to the first aspect.
  • the present invention also provides according to a fourth aspect use of microfibrillated cellulose according to the second or the third aspect in a strength additive, a thickener, a viscosity modifier, a rheology modifier, a cleaning powder, a washing powder, a detergent, a foam composition, a barrier, a film, a food product, a pharmaceutical composition, a cosmetic product, a paper or board product, a coating, a hygiene/absorbent product, an emulsion/dispersing agent, a drilling mud, a composite material , in water purification , in a filter, in a solar cell, in a battery , in an electronic circuit (which may be flexible, printed or coated), or to enhance the reactivity of cellulose in the manufacture of regenerated cellulose or cellulose derivatives.
  • the object of the present invention is thus to provide a process for the dewatering of a a slurry comprising microfibrillated cellulose in an improved way.
  • Another object of the present invention is to provide dewatered microfibrillated cellulose with improved properties.
  • the dewatering may be done by electro-osmosis (or capillary electrophoresis). This dewatering may also additionally also involve ultrasound treatment.
  • the dewatering may also be followed by any one or a combination thereof of the below methods to further dry the material:
  • an electric field with a voltage of 10-100 V is used. Increasing the voltage typically increases the water extraction rate. The optimal value is when the current intensity of the generated electric field and the voltage gradient are at maximum allowable levels.
  • Pressure may also be applied to the slurry in order to further improve the dewatering of the slurry.
  • the pressure may be applied after the electric field has been applied and the dewatering of the slurry has been started. This is due to that it may be preferred to increase the dry content of the slurry before pressure is applied. However, it depends of course on the dry content of the slurry being treated.
  • the pressure applied is preferably a mechanical pressure, such as compression by the use of for example a roll nip or felts.
  • the dry content of the slurry comprising microfibrillated cellulose before dewatering is preferably about 1-10% by weight. After the treatment according to the process it is preferred that the dry content of the dewatered slurry comprising microfibrillated cellulose is about 5-50% by weight.
  • the temperature of the slurry during dewatering is preferably above 30°C and preferably below 100°C.
  • the slurry may also comprise nanoparticles, salt and/or surfactants which are stimulated by the electric field and improves the liquid flow. In this way the dewatering of the slurry is increased.
  • the present invention also relates to microfibrillated cellulose being dewatered according to the process according to the first aspect above. It has been shown that by dewatering a slurry comprising microfibrillated cellulose by the aid of an electric field no or very limited hornification of the microfibrillated cellulosic fibers will occur.
  • the present invention relates to a process for dewatering a slurry comprising microfibrillated cellulose. Due to the characteristics of microfibrillated cellulose fibers, e.g. its size, size distribution and fiber bonds, it is normally very difficult to dewater a slurry comprising microfibrillated cellulose.
  • microfibrillated cellulose being dewatered according to the present process, to swell when the microfibrillated cellulose is in contact with water again.
  • the microfibrillated cellulose for example is used as a strength additive, a thickener or as a viscosity modifier.
  • the bonding ability of the dewatered microfibrillated cellulose is also very good, i.e. no substantial decrease in bonding ability is seen.
  • Electro-osmotic flow is often abbreviated EOF which is synonymous with electro-osmosis or electro-endosmosis.
  • Electro-osmosis is the motion of liquid, such as water, induced by an applied potential or electric field across a porous material, capillary tube, membrane, microchannel, or any other fluid conduit.
  • the voltage generated by the electric field is preferably between 10-100 V.
  • the liquid of the slurry is separated from the microfibrillated cellulose by removing the liquid as set out in the first aspect. It may preferably be done by different filtering techniques.
  • the slurry comprises microfibrillated cellulose and a liquid.
  • the liquid may be water, a solvent and mixtures of different solvents and/or liquids.
  • the solvent may be an alcohol, such as isopropanol, polyethylene glycol, glycol or ethanol. Solvents, such as isopropanol, can change the surface tension of the slurry and this will promote dewatering.
  • the solvent may also be a solvent having at least one ketone group, and this may preferably be acetone. It is also possible that the liquid is an ionic liquid.
  • the slurry may also comprise nanoparticles, salts and/or surfactants which are stimulated by the electric field and will improve the liquid migration and movement, i.e. the flow, in the electric field and thus also the dewatering.
  • the slurry may also comprise fibers of regular length. It is also possible that the slurry comprises fillers, such as PCC, kaolin or calcium carbonate.
  • the amounts of microfibrillated cellulose in the slurry may be between 20-90% by weight, the amount of regular sized fibers such as kraft, hardwood and/or softwood fibers may be 10-80% by weight. If larger amounts of fillers and longer fibers are present in the slurry it is possible to achieve a slurry with very high dry content by using the dewatering process according to the invention. A dry content of up to 90% by weight is possible to achieve since the present of long fibers and/or fillers will make it easier to dewater the slurry.
  • a slurry comprising high amounts of microfibrillated cellulose it is however, preferred to use a slurry comprising high amounts of microfibrillated cellulose.
  • the amount of microfibrillated cellulose depends on the end use of the microfibrillated cellulose.
  • the slurry may also be advantageous to subject the slurry to increased pressure in combination with the electric field. It has been shown that the combination of electric field and pressure will strongly improve the dewatering of a slurry comprising microfibrillated cellulose. It is preferred to apply the pressure after the dewatering with the electric field has started, i.e. when the solid content of the slurry has increased, preferably to about 4% by weight. If the solid content of the slurry is too low when the pressure is applied, the microfibrillated cellulose is pressed through the openings of the dewatering device together with the water and no water/microfibrillated cellulose separation will occur. When the solid content of the slurry is increased, the viscosity is also increased and it is possible to apply pressure to the slurry and be able to increase the dewatering of the slurry.
  • the pressure is preferably a mechanical pressure being applied in any possible way. It possible to use, for example a roll nip or felts for applying the mechanical pressure to the slurry during dewatering. It is also possible to combine the treatment with the electric field with other kind of treatments in order to increase the dewatering. Examples of other treatments besides increasing the pressure are acoustic and vacuum based systems.
  • the dry content of the slurry comprising microfibrillated cellulose before dewatering is preferably about 1-50% by weight. It may also have about 1-30% by weight or about 1-10% by weight.
  • the dry content of the dewatered slurry comprising microfibrillated cellulose is about 5-50% by weight, more preferably above 20% by weight. It is thus possible to receive a slurry comprising microfibrillated cellulose with very high dry content in a very energy efficient way. Even though the dry content is increased the properties of the microfibrillated cellulose after dilution of water is maintained, e.g. the water swelling properties and strength.
  • the temperature of the slurry may be below 30°C before dewatering and increased during the dewatering process but kept at a temperature below 100°C. However, lower temperatures, for example room temperatures are also possible.
  • the temperature should preferably be kept below boiling point. Increased temperature may improve the dewatering. This is due to that that the viscosity of water is decreased.
  • the present invention also relates to microfibrillated cellulose being dewatered according to the first aspect as set out above. It has been shown that by dewatering a slurry comprising microfibrillated cellulose by the aid of an electric field, no or very limited hornification of the microfibrillated cellulosic fibers will occur. It is thus possible to produce a microfibrillated cellulose with improved properties in a fast and very energy efficient way compared to the use of for example drying techniques.
  • a microfibrillated cellulose fiber is normally very thin ( ⁇ 20 nm) and the length is often between 100 nm to 10 ⁇ m. However, the microfibrils may also be longer, for example between 10-200 ⁇ m, but lengths even 2000 ⁇ m can be found due to wide length distribution. Fibers that has been fibrillated and which have microfibrils on the surface and microfibrils that are separated and located in a water phase of a slurry are included in the definition MFC. Furthermore, whiskers are also included in the definition MFC.
  • the microfibrillated cellulose is typically made from wood cellulose fibers, it is possible to use both hardwood and softwood fibers. It can also be made from microbial sources, agricultural fibers, such as wheat straw pulp or other non-wood fiber sources.
  • Fig. 1 For investigation of MFC dispersion dewatering an experimental setup was assembled, scheme of which is on Fig. 1 . It consists of a plastic pipe with internal diameter 46 mm, fitted into a stainless steel funnel. At the lower end of the pipe there is a plate with holes, also made of stainless steel, which serves as the lower electrode, usually cathode. A paper filter is placed on the plate, the MFC dispersion is loaded onto the filter. On top or the MFC column there is one more paper filter, after this the upper electrode (anode) is placed.
  • Fig. 1 constituted a cell with MFC investigated; DC voltage was applied into it from the current source.
  • the water, emerging from the funnel was assembled into beaker, which was situated on top of a balance; the mass of the water extracted from MFC was registered during experiments.
  • the experiments usually were carried out in two modes: with a voltage U constant or with current i constant.
  • Figure 3 discloses dewatering of low conductivity MFC.
  • Figure 4 disclose time dependencies of the water mass collected during dewatering of low conductivity MFC at different voltages are presented.
  • the voltage increase causes an increase of dewatering speed (initial slope) and process saturation value.
  • MFC was dewatered 5 min (as in procedure 1 above i.e. Example 2). After this the current was switched off and acetone was added (about the same amount as water was removed in previous step). After this dewatering was started and continued about 10 min.
  • Dewatered MFC electro-osmosis MFC with acetone

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  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Urology & Nephrology (AREA)
  • Hydrology & Water Resources (AREA)
  • General Chemical & Material Sciences (AREA)
  • Electrochemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Paper (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Medicinal Preparation (AREA)
  • Cosmetics (AREA)
  • Paints Or Removers (AREA)
  • Processing Of Solid Wastes (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Claims (13)

  1. Verfahren zum Entwässern von Schlämme, umfassend mikrofibrillierte Cellulose, wobei das Verfahren die folgenden Schritte umfasst:
    - Bereitstellen einer Schlämme, die mikrofibrillierte Cellulose und Flüssigkeit umfasst,
    - Unterwerfen der Schlämme zu einem elektrischen Feld, das veranlasst, dass die Flüssigkeit der Schlämme fließt, und
    - Trennen der Flüssigkeit von der mikrofibrillierten Cellulose.
  2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, dass das Entwässern durch Elektroosmose erfolgt.
  3. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass ein elektrisches Feld mit einer Spannung von 10 bis 100 V verwendet wird.
  4. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass auch Druck ausgeübt wird, um die Schlämme zu entwässern.
  5. Verfahren nach Anspruch 4, dadurch gekennzeichnet, dass der Druck ausgeübt wird, nachdem das elektrische Feld angewandt und das Entwässern gestartet wurde.
  6. Verfahren nach einem der Ansprüche 4 bis 5, dadurch gekennzeichnet, dass der Druck ein mechanischer Druck ist.
  7. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass der Trockengehalt der Schlämme, die mikrofibrillierte Cellulose umfasst, vor dem Entwässern ungefähr 1 bis 50 Gewichtsprozent beträgt.
  8. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass der Trockengehalt der entwässerten Schlämme, die mikrofibrillierte Cellulose umfasst, ungefähr 5 bis 50 Gewichtsprozent beträgt.
  9. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Temperatur der Schlämme während des Entwässerns über 30 °C und unter 100 °C beträgt.
  10. Verfahren nach einem der vorstehenden Ansprüche, dadurch gekennzeichnet, dass die Schlämme Nanopartikel, Absorbenzien, Salz, freier Zucker und/oder Tenside umfasst, die durch das elektrische Feld stimuliert werden.
  11. Mikrofibrillierte Cellulose, die gemäß dem Verfahren nach einem der Ansprüche 1 bis 10 entwässert ist.
  12. Mikrofibrillierte Cellulose, die durch das Verfahren nach einem der Ansprüche 1 bis 10 erreichbar ist.
  13. Verwenden von mikrofibrillierter Cellulose nach den Ansprüchen 11 oder 12 in einem Stärkezusatzstoff, einem Dickungsmittel, einem Viskositätsmodifizierer, einem Rheologiemodifizierer, einem Reinigungspulver, einem Waschmittel, einem Reinigungsmittel, einer Schaumzusammensetzung, einer Barriere, einem Film, einem Nahrungsmittelprodukt, einer pharmazeutischen Zusammensetzung, einem Kosmetikprodukt, einem Papier- oder Kartonprodukt, einer Beschichtung, einem Hygiene-/Absorbensprodukt, einem Emulsions-/Dispergiermittel, einem Bohrschlamm, einem Verbundmaterial, bei der Wasseraufbereitung, in einem Filter, in einer Solarzelle, in einer Batterie, in einer elektronischen Schaltung oder um die Reaktivität von Cellulose bei der Herstellung von regenerierter Cellulose oder Cellulosederivaten zu verbessern.
EP12786645.7A 2011-05-13 2012-05-11 Verfahren zur behandlung mikrofibrillierter cellulose und in diesem verfahren behandelte mikrofibrillierte cellulose Active EP2707540B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
SE1150436 2011-05-13
PCT/IB2012/052351 WO2012156880A1 (en) 2011-05-13 2012-05-11 Process for treating microfibrillated cellulose and microfibrillated cellulose treated according to the process

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EP2707540A1 EP2707540A1 (de) 2014-03-19
EP2707540A4 EP2707540A4 (de) 2014-11-19
EP2707540B1 true EP2707540B1 (de) 2016-07-13

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EP12786645.7A Active EP2707540B1 (de) 2011-05-13 2012-05-11 Verfahren zur behandlung mikrofibrillierter cellulose und in diesem verfahren behandelte mikrofibrillierte cellulose

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EP (2) EP2707541B1 (de)
JP (2) JP6165715B2 (de)
CN (2) CN103534409B (de)
AU (2) AU2012257467B2 (de)
BR (2) BR112013029109B1 (de)
CA (2) CA2835302C (de)
CL (2) CL2013003259A1 (de)
DK (2) DK2707541T3 (de)
ES (2) ES2596216T3 (de)
PL (2) PL2707540T3 (de)
RU (2) RU2603957C2 (de)
WO (2) WO2012156882A1 (de)
ZA (2) ZA201308337B (de)

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US20140073774A1 (en) 2014-03-13
US9447541B2 (en) 2016-09-20
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EP2707540A1 (de) 2014-03-19
ES2596227T3 (es) 2017-01-05
EP2707541A4 (de) 2014-11-19
AU2012257465B2 (en) 2017-05-04
EP2707541A1 (de) 2014-03-19
BR112013029110A2 (pt) 2017-02-07
RU2603956C2 (ru) 2016-12-10
PL2707541T3 (pl) 2017-01-31
RU2603957C2 (ru) 2016-12-10
EP2707540A4 (de) 2014-11-19
CA2835302C (en) 2019-10-22
EP2707541B1 (de) 2016-07-13
JP2014514427A (ja) 2014-06-19
BR112013029109A2 (pt) 2017-02-07
CN103534408B (zh) 2016-04-06
US20140088301A1 (en) 2014-03-27
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BR112013029110B1 (pt) 2021-07-27
PL2707540T3 (pl) 2016-12-30
CA2834460A1 (en) 2012-11-22
RU2013155187A (ru) 2015-06-20
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